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Separation method of polyamide-amine dendritic compound

A technology of amine dendritic and separation method, which is applied in the field of polymer material preparation, can solve the problem of insufficient separation of reaction materials and solvents, and achieve obvious effects and reduce the residual amount

Pending Publication Date: 2018-03-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to improve the vacuum distillation operation process aimed at reducing the residual amount of reaction material and solvent in the PAMAM product in the PAMAM product after vacuum distillation in the current PAMAM preparation process.

Method used

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  • Separation method of polyamide-amine dendritic compound
  • Separation method of polyamide-amine dendritic compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Separation and purification of semi-algebraic PAMAM G0.5: after the Michael addition reaction of semi-algebraic G0.5 preparation, it is divided into 2 parts for vacuum distillation. One part, using the semi-algebraic Michael addition reaction product vacuum distillation process (see attached figure 1 ), the specific process includes initial distillation (1.1), primary vacuum distillation (1.2) using solvent extraction, secondary vacuum distillation (2.2) using fresh methanol as extraction solvent, and the yield of the final product G0.5 is 98.8 %. Another part, using the conventional vacuum distillation process, that is, the initial distillation (1.1) process, but the operating parameters are temperature 50 ° C, vacuum ~ 101 kPa, the yield of product G0.5 is 99.2%. The method described in this patent application is more thoroughly separated than conventional methods.

[0037] Yield = product obtained by distillation under reduced pressure ÷ the amount of product obtai...

Embodiment 2

[0039] Separation and purification of semi-algebraic PAMAM G2.5: After the Michael addition reaction of semi-algebraic G2.5 is prepared, it is divided into two parts for vacuum distillation. One part, using the semi-algebraic Michael addition reaction product vacuum distillation process (see attached figure 1 ), the specific procedures include initial distillation (1.1), primary vacuum distillation using solvent extraction (1.2), secondary vacuum distillation (2.2) using fresh methanol as extraction solvent, and final vacuum distillation (temperature 54°C , vacuum ~101kPa), the yield of the final product G2.5 is 95.4%. The other part, using the conventional vacuum distillation process, that is, the initial distillation (1.1) process, but the operating parameters are temperature 50 ° C, vacuum ~ 101 kPa, the yield of the obtained product G2.5 is 105.3%. Excess reactant MA and solvent still obviously remain in the product obtained by the conventional method, but the method desc...

Embodiment 3

[0041] Separation and purification of semi-algebraic PAMAM G3.5: After the Michael addition reaction of semi-algebraic G3.5 was prepared, it was divided into two parts for vacuum distillation. One part, using the semi-algebraic Michael addition reaction product vacuum distillation process (see attached figure 1 ), the specific procedures include initial distillation (1.1), primary vacuum distillation using distillate as extraction solvent (1.2) and (1.3), secondary vacuum distillation using distillate and fresh methanol as extraction solvent (2.1) and (2.2), final vacuum distillation (temperature 54°C, vacuum ~101kPa), that is, the entire process of separation of Michael reaction products mentioned above in this patent application, the yield of the final product G3.5 is 97.7%. The other part, using the conventional vacuum distillation process, that is, the initial distillation (1.1) process, but the operating parameters are temperature 50 ° C, vacuum ~ 101 kPa, the yield of th...

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Abstract

The invention relates to an improvement in a vacuum distillation method used for purification and separation in the preparation process of a polyamide-amine (PAMAM) dendritic compound. A separation method of the polyamide-amine dendritic compound is characterized in that as for vacuum distillation taking ethidenediamine (EDA) and methyl acrylate (MA) as reaction raw materials, and methanol as a reaction solvent in the PAMAM preparation process, after the Michael addition excess reaction and amidation excess reaction are finished, a secondary vacuum distillation process is respectively implemented according to different temperatures and vacuum degrees, and 1-3 solvent extraction operations are added in each stage; the separation of a target product from an excess reactant is enhanced through solvent extraction, so that the separation time is shortened. The separation method of the polyamide-amine dendritic compound, provided by the invention, has the beneficial effects that operation procedures and operating parameters for the vacuum distillation reasonably utilize the demands of the distillation temperatures, the vacuum degrees and methanol as the reaction solvent at different stages of vacuum distillation and purification of PAMAM reaction material liquid, the residual amount of reaction materials in the target PAMAM product is reduced, and particularly, the effect is more obvious along with the increase of PAMAM algebras.

Description

technical field [0001] The invention relates to a purification and separation method in the preparation process of polyamide-amine dendrons, and belongs to the technical field of polymer material preparation. Background technique [0002] Polyamidoamine dendrimers (PAMAMs) are widely studied dendrimers. PAMAM has good compatibility, thermal stability, low melt viscosity and solution viscosity, unique hydrodynamic properties and easy modification, which makes it show in drug control release, material modification, nanomaterials, functional catalysis, etc. a great application prospect. [0003] Regarding the preparation of PAMAM, similar methods are basically adopted at home and abroad, the synthetic reaction is carried out by the divergent method, and the product, the unconsumed reactant and the solvent are separated by vacuum distillation. The divergent synthesis of PAMAM generally uses multifunctional substances such as ethylenediamine (EDA), hexamethylenediamine, and ami...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00
CPCC08G83/004
Inventor 毛松柏周志斌朱道平
Owner CHINA PETROLEUM & CHEM CORP
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